节点文献
1,4-二(2′,6′-二异丙基苯基)-2,2,5,5-四甲基-1,4-二氮杂-2,5-二硅杂环己烷的合成、表征及其晶体结构
Synthesis and Crystal Structure of 1,4-bis(2′,6′-diisopropylphenyl)-2,2,5,5-tetramethyl-1,4-diaza-2,5-disilacyclohexane
【摘要】 用2,6-二异丙基苯胺2,6i-Pr2C6H3NH2与1当量的n-BuLi在乙醚溶液中-78℃条件下反应,以98%的产率得到2,6i-Pr2C6H3NHLi(1).用化合物1以当量比1:1与ClSiMe2CH2Cl冰水浴条件下反应,得到1,4-二(2′,6′-二异丙基苯基)-2,2,5,5-四甲基-1,4-二氮杂-2,5-二硅杂环己烷.产物经1H NMR,IR,其晶体结构经X-射线单晶衍射分析确证.晶体属单斜晶系,空间群P21/n,晶胞参数:a=8.4917(2),b=11.2259(2),c=16.2409(2);α=90°,β=98.4080°,γ=90°;V=1531.56(4)3,T=293K,Z=2,Dc=1.073mg/m3,μ=0.135mm-1,λ=0.71073,F(000)=544,结构偏离因子R=0.0402,wR=0.1197,共收集到7610个独立衍射点,其中I>2σ(I)的可观测点为3462个.
【Abstract】 Reaction of 2,6-iPr2C6H3NH2 with 1 equiv of n-BuLi in Et2O at-78℃ yielded2,6-iPr2C6H3NHLi(1) in 98% yield.Treatment of ClSiMe2CH2Cl with 1 equiv of 1 in Et2O at 0℃ for 24 hours,after recrystallization from hexane,gave the compound 1,4-bis(2′,6′-diisopropylphenyl)-2,2,5,5-tetramethyl-1,4-diaza-2,5-disilacyclohexane.The compound was characterized by 1H NMR and IR.The single crystal structure was determined by X-ray diffraction analysis.Crystal crystallizes in monoclinic,space group P2(1)/n with unit cell parameters: a=8.49170(10),b=11.2259(2) ,c=16.2409(2)?;α=90°,β=98.4080,γ=90;V=1531.56(4)?3,T=293K,Z=2,Dc=1.073mg/m3,μ=0.135mm-1,λ=0.71073?,F(000)=544.The final R=0.0402,wR=0.1197,7610 independent were collected,of which 3462 independent reflections with I>2σ(I) were used.
【Key words】 synthesis; 1,4-diaza-2,5-disila cyclohexane; crystal structure;
- 【文献出处】 安徽师范大学学报(自然科学版) ,Journal of Anhui Normal University(Natural Science) , 编辑部邮箱 ,2008年05期
- 【分类号】O627.41
- 【下载频次】83